利用富铈混合稀土改善工业纯铝中富铁相形貌的研究

利用金相分析方法研究了富Ce混合稀土变质对含不同Fe量的工业纯铝的组织和其中富铁相形貌的影响。试验结果表明,随着Fe含量的增加,富铁相由弥散细小的颗粒状向短棒状、长针状转变;富Ce混合稀土变质使铝中的富铁相由长针状变为弥散细小的颗粒状。随着稀土含量的增加,-αAl晶粒逐渐细化,富铁相尺寸及数量逐渐减小。添加0.5%稀土时,-αAl晶粒细化效果最佳,而且富铁相呈细小颗粒状均匀分布在-αAl基体的晶界处。本文还对稀土改善富铁相的机制进行了分析。     

CreditRisk+模型下商业银行经济资本配置研究

对金融资产风险的度量与经济资本的分配应该体现分散化效应,传统的V aR方式不能保证分散化效应的次可加性.本文讨论了基于T a ilV aR这一新的风险度量与经济资本分配标准,并在违约率均值不变情况下,对C red itR isk+模型下的商业银行经济资本分配进行了实证分析.     

基于人工神经网络的商业银行信用风险模型

在对人工神经网络的基本原理进行简要介绍的基础上 ,着重对构建商业银行信用风险的人工神经网络模型进行了研究 ,实证结果表明 ,人工神经网模型具有很高的预测精度     

Chemiluminescence Determination of Benzoic Acid Using A Solid-Phase Verdigris Reactor

Benzoicacidisacommonadditiveusedwidelyasfoodpreservativeandplasticizer.Itcouldpromoteseverereactiontoallergicpopulationevenatlowconcentrationlevel1.Routinemethodsfortheassayofbenzoicacidincludeschromatographic2-6,spectrophotometry7,8,capillaryelectrophoresis9-13andelectrochemicaltitration14.Stokes15etal.monitoredairbornebenzoicacidbasedonsurface-enhancedRamanscatteringtechniques.Thereisalsoreportonamicrobialsensorusingpseudomonasforbenzoicacidandtheirderivativesinaqua16.Interestofusinglumines…     

Electrochemical Evaluation of Nucleoside Analogue Lamivudine in Pharmaceutical Dosage Forms and Human Serum

Lamivudine (LAM) is a synthetic nucleoside analogue with activity against human immunodeficiency virus‐type 1 (HIV‐1) and Hepatitis B virus (HBV). The aim of this study was to determine LAM levels in serum and pharmaceutical formulations, by means of electrochemical methods using hanging mercury drop electrode (HMDE). On this electrode, LAM undergoes irreversible reduction at the peak potential near E_p?1.26 V (vs. Ag/AgCl/3 M KCl). Reduction LAM signals were measured by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and square‐wave voltammetry (OSW). DPV and OSW techniques for the determination of LAM in acetate buffer at pH 4.5, which allows quantitation over the 4×10^?6 to 1×10^?4 M range in supporting electrolyte for both methods, were proposed. The linear response was obtained in acetate buffer in the ranges of 2×10^?6 to 2×10^?4 M for spiked serum samples at pH 4.5 for both techniques. The repeatability and reproducibility of the methods for all media were determined. The standard addition method was used in serum. Precision and accuracy were also checked in all media. No electroactive interferences from the endogenous substances were found in serum. With respect to side effects of high doses and short half‐life of LAM, a fast and simple detection method is described in this study.     

Solid sampling Fourier transform infrared determination of Mancozeb in pesticide formulations

A series of approaches have been assayed for FTIR determination of Mancozeb in several solid commercial fungicides using different calibration strategies. The simplest procedure was based on the use of the ratio between the absorbance of a characteristic band of Mancozeb and that of a KSCN internal standard measured in the FTIR spectra obtained from KBr pellets. It was employed the quotient between peak height absorbance values at 1525 cm⁻¹ for Mancozeb and 2070 cm⁻¹ for KSCN. In these conditions a precision as relative standard deviation (RSD) of 0.6% and a relative accuracy error of 0.8% (w/w) were found. For complex formulations, containing other compounds with characteristic absorption bands at different wavenumbers than Mancozeb, one of them was used as internal reference being employed the standard addition approach. In this case, the Mancozeb bands at 1525 cm⁻¹ or at 1289 cm⁻¹ were employed, being used the ferrocyanide band at 2075 cm⁻¹ as internal reference. RSD values between 0.7-1.4% and a relative accuracy error of 3% (w/w) were found. A third strategy was based on the use of partial least squares (PLS) calibration. A reference set was prepared mixing Mancozeb, Kaolin, Cymoxanil and KBr, being predicted the Mancozeb concentration in pesticide formulations by using the quotient between absorbance bands of Mancozeb and those of Cymoxanil. In these conditions a relative accuracy error of 0.6% (w/w) and a relative standard deviation of 1.3% were found.     

Compatibility Studies of Multicomponent Tablet Formulations. DSC and experimental mixture design

An experimental mixture design was applied to a differential scanning calorimetry (DSC) study performed to evaluate naproxen compatibility in tablet formulations consisting of four classic excipients (sorbitol, sodium carboxymethylcellulose, poly(ethylene glycol) 20000 and Veegum) each in adequate concentration ranges accounting for the relevant values actually used in pharmaceutical formulations. Twenty-seven different tablets were obtained from as many mixtures prepared according to the experimental design plan and analyzed in a random order by DSC. Statistical evaluation of experimental data enabled correlation of both enthalpy and onset temperature variations of drug melting endotherm (selected as responses indicative of the presence of drug-excipient interactions) with the mixture composition. Variance analysis (Anova) confirmed the reliability of the postulated polynomial model in providing adequate prediction of true system behaviour. This revised version was published online in August 2006 with corrections to the Cover Date.     

Application of heat conduction calorimetry to high explosives

This paper describes some thermal analysis experiments conducted on high explosive samples. These employ differential scanning calorimetry to monitor thermal effects at elevated temperatures (around 200 °C) and heat conduction calorimetry to record thermal effects at much lower temperatures (below 100 °C).The work shows that, due to the generally high thermal stability of many high explosive compositions, heat generation rates are very low, if detectable at all, at normal storage temperatures, even when using a very sensitive instrument. The sensitivity and reproducibility of this technique has been investigated in detail by Wilker et al. [S. Wilker, U. Ticmanis, G. Pantel, Detailed investigation of sensitivity and reproducibility of heat flow calorimetry, in: Proceedings of the 11th Symposium on Chemical Problems Connected with the Stability of Explosives, Sweden, 1998] and shown to be capable of recording heat generation rates of less than a microwatt. This allows continuous measurement of decomposition processes in nitrate ester based propellants at temperatures as low as 40 °C. However, the measurement of very low levels of heat generation is difficult, time consuming and therefore expensive. If the assumption is made that the life limiting process is invariably the slow decomposition of the energetic component, this will frequently lead to very long service lifetime predictions.A number of possible complications are identified. Firstly, due to its low detection threshold, a heat conduction calorimeter may detect other reactions which will not lead to failure, but which may still dominate the heat flow signal. Secondly, the true failure process may generate little energy and be overlooked. In view of these considerations, at present it seems unwise to rely on heat conduction microcalorimetry as the only tool for the assessment of the life of high explosive energetic systems.Based on examples of life terminating processes in high explosives during storage and use, it is clear that decomposition of the energetic material is not invariably the cause of system failure. It is also by no means the only reaction that may take place in, and be observed by, a heat conduction calorimeter.     

HPLC determination of pyroglutamic acid as a degradation product in parenteral amino acid formulations

Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects.Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur.The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 m Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5.Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce.     

FIA-fluorimetric determination of adrenaline in pharmaceutical formulations by oxidation with molecular oxygen

The fluorimetric determination of adrenaline is carried out in a continuous-flow assembly and by means of the molecular dissolved oxygen. The sample solution merges with an NaOH stream, then the resulting mixture is heated at 73 °C and led to the flow-cell of the fluorimeter. The flow-assembly is very simple and the procedure is quick (107 samples h^–1) reproducible (R.S.D. 0.6%), selective and suitable to be applied to determination of adrenaline in formulations. Calibrations graph are linear over the ranges 0.05–15 and 20–40 mgl^–1.